CN106206082A - There is the preparation method and application of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic - Google Patents

There is the preparation method and application of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic Download PDF

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CN106206082A
CN106206082A CN201610696733.2A CN201610696733A CN106206082A CN 106206082 A CN106206082 A CN 106206082A CN 201610696733 A CN201610696733 A CN 201610696733A CN 106206082 A CN106206082 A CN 106206082A
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electrode
graphene
nickel oxide
nickel
combination electrode
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CN106206082B (en
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孙伟
王文成
李小宝
牛学良
闫丽君
文作瑞
陈玮
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Hainan Normal University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/26Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H01G11/28Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses the preparation method and application of the nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic, it is prepared for nickel oxide and graphene composite material modified electrode for substrate substep electrodeposition process with nickel foam, by scanning electron microscope, nickel oxide/graphene composite material is carried out morphology characterization, result display graphene film is close to nickel foam surface, and nickel oxide nano sheet uniform load is on graphene film.By electrochemical method, the capacitive property of described combination electrode is tested, result shows that the chemical property of nickel oxide/graphene combination electrode is greatly improved compared with graphene modified electrode, and charge-discharge test shows that nickel oxide/graphene combination electrode is at 1 mA/cm2Ratio electric capacity under electric current density is 381 mF/cm2, illustrate that nickel oxide/graphene composite material is a kind of good super capacitor material.

Description

There is the preparation method of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic And application
Technical field
The present invention relates to preparation and the test of capacitive property thereof of a kind of ultracapacitor combination electrode.
Background technology
Along with exhaustion and the appearance of ecological deterioration problem of traditional energy, about cleaning, efficient, novel, regenerative resource The research of material and device and application are constantly subjected to the extensive attention of researcher.Easily it is transmitted owing to electric energy has and utilizes Feature, be far superior to other various forms of energy, so how make full use of electric energy and just become extremely important.In this background Under all kinds of electrochmical power sources arise at the historic moment, such as fuel cell, lithium ion battery and ultracapacitor etc..Compared with ordinary capacitor The energy density of ultracapacitor is higher, and compared with lithium battery, the power density of ultracapacitor is higher, in addition ultracapacitor Also there is the advantages such as good cycling stability, charge/discharge rates is fast, specific capacitance is big, environmental pollution is little, therefore ultracapacitor Have wide practical use in multiple fields such as new-energy automobile, solar power system, military equipments.
Ultracapacitor can be divided into double electric layers supercapacitor and the super electricity of fake capacitance by the difference according to energy storage mechnism Container.Double layer capacitor is double electrode layer theory based on Helmholtz and grows up, and has compared with ordinary capacitor Charge layer more closely, it is provided that higher capacitance.The electrode material of fake capacitance ultracapacitor usually has greatly The electroactive material of specific surface area, there is the redox reaction of Rapid reversible in the electrolytic solution in these materials, thus at electrode Surface completes storage and the release process of a large amount of electric charge.
Electrode material be affect ultracapacitor capacitive character can principal element, exploitation high-capacitance electrode material for Improve ultracapacitor capacitive character and can have pivotal role.Transition metal oxide is a kind of energy storage material received much concern, its Energy density is higher than the energy density of double layer capacitor.That studies the earliest has metal oxide containing precious metals such as ruthenium-oxide, yittrium oxide etc., Show splendid fake capacitance performance, but it is expensive, limit actual application.Base metal oxide also has preferable electricity Capacitive energy, common are manganese oxide, nickel oxide, cobalt oxide etc..Wherein nickel have wide material sources, preparation cheap, easy and Theoretical ratio electric capacity advantages of higher, is a kind of ideal fake capacitance material.
Graphene has the features such as high conductivity, good mechanical property and bigger serface, is possible not only to surpass as electric double layer The ideal electrode material of level capacitor, is also the preferable base material of fake capacitance ultracapacitor.Graphene is super at fake capacitance The reason that can improve composite capacitive property in capacitor application has: (1) Graphene in the composite makees load matrix Time, the fake capacitance active substance of nanoscale can be distributed in graphenic surface with stable and uniform, substantially increase active matter The electro-chemical activity of matter and utilization rate;(2) Graphene can play the effect of electron channel, by Graphene and fake capacitance activity Contact good between material, can occur quick electric transmission in the composite;(3) unique planar structure of Graphene Contribute to the STRUCTURE DECOMPOSITION limiting fake capacitance active substance during ion embeds/departs from, thus improve composite Stability.
The present invention utilizes nickel foam loose structure can improve the advantage of electrode specific surface area, using it as combination electrode Collector, obtains grapheme material by potentiostatic electrodeposition method, then is being modified with Graphene material by electrochemical process on its surface The collection liquid surface electro-deposition of material obtains nickel oxide nano sheet, successfully prepares nickel oxide/graphene combination electrode, by scanning Its microscopic appearance is characterized by Electronic Speculum, electrochemically tests its capacitive property.
Summary of the invention
It is an object of the invention to announce the preparation method of the nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic And application process, concrete grammar is: utilizes potentiostatic method to have relatively high electrochemical in the control synthesis of nickel foam collection liquid surface and lives Property graphene film, further electrochemical deposition prepares nickel oxide/graphene combination electrode that capacitive property is excellent.By sweeping Retouch Electronic Speculum evaluate prepared by the shape characteristic of combination electrode, nickel foam collector has uniformly been coated with a layer graphene and in Reveal the NiO nanometer sheet being evenly distributed.Build three-electrode system with described combination electrode for working electrode, pass through cyclic voltammetric Method, AC impedence method and constant current charge-discharge method test the capacitive property of described combination electrode.Result shows described combination electrode There is under high current density the highest energy density and excellent high rate performance, show equally in cycle charge discharge electrical testing Splendid cyclical stability, illustrates that nickel oxide/graphene combination electrode has potential using value in ultracapacitor field.
Nickel oxide/graphene combination electrode is by nickel foam collector (basal layer), Graphene (intermediate layer) and NiO nanometer sheet (outer layer) is constituted.
Described Graphene forms ultra-thin tight clad at nickel foam collection liquid surface.
Described NiO nanometer sheet homoepitaxial is at graphenic surface, it is possible to be effectively improved the specific surface area of combination electrode.
A kind of method preparing nickel oxide/graphene combination electrode, with nickel foam collector as basal layer, utilizes constant potential Sedimentation obtains graphene interlayers in substrate surface electro-deposition, then powers at graphene interlayers by two step cyclic voltammetries Deposition obtains NiO nanometer sheet outer layer, and its concrete preparation process is as follows:
1) nickel foam is cut into the square of certain size, successively with acetone, certain density hydrochloric acid solution ultrasonic cleaning one Fix time and number of times, be carried out with distilled water afterwards, then with ethanol rinse, finally dry up with nitrogen standby;
2) in the PBS of certain pH, a certain amount of graphene oxide of ultrasonic disperse obtains homogeneous suspension, after deoxygenation With above-mentioned suspension as electrolyte, nickel foam collector (NF) is working electrode, builds three-electrode system, at nickel foam collector Surface utilizes potentiostatic method deposition to obtain Graphene, and taking-up distilled water obtains GR/NF after cleaning, standby after vacuum drying;
3) dissolve nickel nitrate with the acetate buffer solution of certain pH and configure certain density nickel nitrate solution, molten with above-mentioned nickel nitrate Liquid is electrolyte, works electrode with GR/NF electrode, builds three-electrode system.Utilize two step cyclic voltammetries at GR/NF electrode The NiO nanometer sheet that surface electro-deposition is evenly distributed, cleans with distilled water after taking-up and obtains nickel oxide/Graphene compound electric Pole, is denoted as NiO/GR/NF, standby after vacuum drying;
4) with KOH as electrolyte, NF, GR/NF, NiO/GR/NF with the preparation of step 1, step 2 and step 3 are electric for work respectively Pole, builds three-electrode system, by cyclic voltammetry and constant current charge-discharge method test above-mentioned working electrode capacitive property.
The size of the square nickel foam stated in step 1 is 1 cm × 1 cm;The nickel foam hole stated in step 1 Gap rate is more than 90%;The nickel foam pore diameter range stated in step 1 is 1 mm ~ 10 mm;The hydrochloric acid solution stated in step 1 Concentration be 3.0 mol/L;The every kind of solution ultrasonic cleaning number of times stated in step 1 is 3 times, the time of each ultrasonic cleaning It is 10 min.
The pH of the PBS buffer solution stated in step 2 is 8.0;The concentration of the graphene oxide stated in step 2 is 1.0 mg/mL;The deoxidation method stated in step 2 is to be passed through a certain amount of nitrogen;Three electricity of the structure stated in step 2 Electrode systems includes: working electrode (nickel foam collector), reference electrode (saturated calomel electrode), auxiliary electrode (platinum plate electrode); The potentiostatic electrodeposition method stated in step 2 prepares the condition of Graphene: sedimentation potential is-1.2 V, and sedimentation time is 600 s;The distilled water stated in step 2 is redistilled water.
The pH of the acetate buffer solution stated in step 3 is 4.0;The concentration of the nickel nitrate solution stated in step 3 is 1.0 mmol/L;The three-electrode system stated in step 3 be working electrode (GR/NF), reference electrode (saturated calomel electrode), Auxiliary electrode (platinum plate electrode);The first step cyclic voltammetry sedimentary condition stated in step 3: be with above-mentioned nickelous nitrate solution Electrolyte, potential window is-1.0 V~0.5 V, and scanning speed is 70 mV/s, and the scanning number of turns is 30 circles;Step 3 is stated Second step cyclic voltammetry sedimentary condition: with complete first step cyclic voltammetry deposition reaction electrode as working electrode, with The PBS solution of pH 7 is electrolyte, and potential window is-1 V~1.5 V, and scanning speed is 100 mV/s, and the scanning number of turns is 30 Circle.
The concentration of the KOH solution stated in step 4 is 1.0 mol/L;Reference in the three-electrode system that step 4 is stated Electrode be hydrargyrum/mercuric oxide electrode, auxiliary electrode be platinum plate electrode;The potential range of the cyclic voltammetry stated in step 4 Being 0~0.8 V, scanning speed is 5,10,20,30,50,80,100,150 mV/s;The permanent electricity stated in step 4 The potential range of stream charge-discharge test is 0~0.5 V, and electric current density is 1,2,3,5,10,20,40 mA/cm2
The invention has the beneficial effects as follows: the present invention proposes one and simply prepares nickel oxide/graphene combination electrode and survey The method trying this combination electrode capacitive property.Utilize potentiostatic electrodeposition method to control synthesis at nickel foam collection liquid surface and have higher The graphene film of electro-chemical activity, further electrochemical synthesis has the NiO nanometer sheet of outstanding capacitive property, builds oxidation Nickel/graphene combination electrode.Electrochemical method is prepared the method for Graphene and NiO nanometer sheet and is had simple and convenient, quick and green The free of contamination feature of color.Nickel oxide/graphene combination electrode prepared by the present invention, can give full play to reticulated polymer foam nickel specific surface Long-pending big feature, can be that electric transmission provides express passway, beneficially electronics after collection liquid surface tight coated graphite alkene Absorption and desorption process.Described combination electrode can effectively overcome the shortcoming that NiO internal resistance is bigger, gives full play to NiO nanometer sheet Fake capacitance amount, strengthens the capacitive property of combination electrode.Result of the test shows that nickel oxide/graphene combination electrode has good following Ring stability and higher energy density, can have potential using value as the working electrode of ultracapacitor.
Accompanying drawing explanation
Fig. 1: (A) nickel foam (NF), (B) Graphene/nickel foam (GR/NF), (C) nickel oxide/Graphene/nickel foam (NiO/GR/NF) scanning electron microscope (SEM) photograph (illustration is partial enlarged drawing) of combination electrode.
Fig. 2: the cyclic voltammetry curve of different operating electrode (a → c:NF, GR/NF, NiO/GR/NF), illustration is following of NF Ring volt-ampere curve enlarged drawing, electrolyte is 1.0 mol/L KOH, scanning speed 100 mV/s, and potential window is 0~0.8V.
Fig. 3: the nickel oxide/Graphene/nickel foam not obtained under the synsedimentary number of turns (a → e:5,10,40,20,30) is combined Electrode, in 1.0 mol/L KOH solution, scanning speed is the cyclic voltammetry curve (A) of 100 mV/s;10 mA/cm2Electricity Under charging and discharging curve (B) under current density and not the synsedimentary number of turns than capacitance variations curve (C).
Fig. 4: nickel oxide/Graphene/nickel foam combination electrode in 1.0 mol/L KOH solution different scanning speed (a → H:5,10,20,30,50,80,100,150 mV/s) under cyclic voltammetry curve.
Fig. 5: nickel oxide/Graphene/nickel foam combination electrode different electric current densities (a → g:1,2,3,5,10,20,40 mA/cm2Discharge curve (A) under) and than capacitance variations curve (B).
Fig. 6: nickel oxide/Graphene/nickel foam combination electrode is 10 mA/cm in electric current density2Under conditions of follow for 1000 times Ring discharge and recharge is than capacitance variations curve, and illustration is part cycle charge-discharge curve.
Detailed description of the invention
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but the most therefore and Limit the scope of the invention.
Material and instrument employed in following example are commercially available.
Embodiment 1
Nickel foam collector pretreatment: nickel foam is cut into the square of 1 cm × 1 cm, is then sequentially placed into acetone and 3.0 In the hydrochloric acid of mol/L, ultrasonic 3 times of difference, each 10 min, use dehydrated alcohol drip washing with redistilled water, finally after thoroughly washing Drying up vacuum with nitrogen to save backup, the morphology characterization of nickel foam collector is shown in Fig. 1 (A).
Embodiment 2
PBS 25 mL of configuration pH 8.0, is subsequently adding 25.0 mg graphene oxides, obtains steady after ultrasonic disperse is uniform 1.0 fixed mg/mL graphene oxide suspension, with it as electrolyte, nickel foam collector is working electrode, saturated calomel electricity Extremely reference electrode, platinum plate electrode is that auxiliary electrode builds three-electrode system, at sedimentation potential-1.2 V and sedimentation time 600 s Under conditions of, obtain being coated with close graphene film at nickel foam collection liquid surface by potentiostatic electrodeposition method, the stone of preparation Ink alkene modified electrode is denoted as GR/NF, and morphology characterization is shown in Fig. 1 (B).
Embodiment 3
Configure the nickel nitrate solution of 1.0 mmol/L with the acetate buffer solution of pH 4.0, with it as electrolyte, be work with GR/NF Electrode, saturated calomel electrode is reference electrode, and platinum plate electrode is that auxiliary electrode builds three-electrode system.Complete by cyclic voltammetry Becoming first step electrodeposition process, sedimentary condition: potential window scope is-1.0 V~0.5 V, scanning speed is 70 mV/s, sweeps Retouching the number of turns is 30 circles.Completing second step process by cyclic voltammetry, experiment condition is: to complete first step cyclic voltammetry Electrode is working electrode, and saturated calomel electrode does reference electrode, and platinum plate electrode does auxiliary electrode and builds three-electrode system, with pH The PBS solution of 7.0 is electrolyte, and potential window is-1.0 V~1.5 V, and scanning speed is 100 mV/s and the scanning number of turns is 30 Circle.The NiO nanometer sheet being evenly distributed in the electro-deposition of GR/NF surface by two step cyclic voltammetries, uses distilled water after taking-up Cleaning obtains nickel oxide/Graphene/nickel foam combination electrode, and its morphology characterization is shown in Fig. 1 (C), is denoted as NiO/GR/NF, and vacuum is done Dry rear standby.
Embodiment 4
With 1.0 mol/L KOH as electrolyte, respectively with NF, GR/NF and NiO/GR/NF for working electrode, hydrargyrum/mercuric oxide electrode For reference electrode, platinized platinum is that auxiliary electrode builds three-electrode system, sets potential window as 0~0.8 V, and scanning speed is 0.1 V/s, tests the capacitive property of above-mentioned working electrode by cyclic voltammetry, and result of the test is shown in Fig. 2.
Embodiment 5
On the basis of embodiment 3, only the scanning number of turns in first step cyclic voltammetric electrodeposition process is adjusted to 5,10,20, 30,40 circles, remaining condition is identical prepares corresponding modified electrode.With 1.0 mol/L KOH as electrolyte, not synsedimentary Under the conditions of preparation nickel oxide/Graphene/nickel foam combination electrode be working electrode, hydrargyrum/mercuric oxide electrode is reference electrode, platinum Sheet is that auxiliary electrode builds three-electrode system, and potential window is 0~0.8 V, and scanning speed is that 100 mV/s pass through cyclic voltammetric Method is tested the capacitive property of above-mentioned working electrode and contrasts, and result of the test is shown in Fig. 3 (A);Potential range 0~0.5 V, electricity Current density is 10 mA/cm2Under conditions of by combination electrode electricity under sedimentary conditions different described in constant current charge-discharge CURVE STUDY The change of capacitive energy, result of the test is shown in Fig. 3 (B).
Embodiment 6
With 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and hydrargyrum/mercuric oxide electrode is reference electrode, platinized platinum Electrode is that auxiliary electrode builds three-electrode system, and potential window is 0~0.8 V, changes scanning speed and is followed successively by 5,10,20, 30,50,80,100,150 mV/s, record cyclic voltammetry curve, see Fig. 4, and then research scanning speed contrast capacitance variations Impact,.
Embodiment 7
With 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and hydrargyrum/mercuric oxide electrode is reference electrode, platinized platinum Electrode is that auxiliary electrode builds three-electrode system, and potential window is 0~0.5 V, and electric current density is respectively 1,2,3,5,10, 20, 40 mA/cm2Under conditions of by constant current charge-discharge CURVE STUDY difference electric current density to described combination electrode capacitive character The impact of energy, result of the test is shown in Fig. 5 (A) and (B).
Embodiment 8
With 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and hydrargyrum/mercuric oxide electrode is reference electrode, platinized platinum Electrode is that auxiliary electrode builds three-electrode system, and potential window is 0~0.5 V, electric current density 10mA/cm2Under conditions of carry out 1000 cycle charge discharge electrical testings, test result is shown in Fig. 6.
First the present invention carries out pretreatment to nickel foam collector, recycling electrochemical method prepare nickel oxide/Graphene/ Nickel foam combination electrode, scanning electron microscope display Graphene is closely coated with nickel foam and forms three-dimensional netted macroscopic body, and its surface is equal Even distribution NiO nanometer sheet.Contrasting the capacitive property of NF, GR/NF and NiO/GR/NF the most respectively, result shows the electricity of NiO/GR/NF Capacitive preferably, and can carry out electro-chemical test to nickel oxide/Graphene/nickel foam combination electrode, result display nickel oxide/graphite Alkene/nickel foam combination electrode has good capacitive property as the working electrode of ultracapacitor.

Claims (5)

1. there is the preparation method and application of the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic, including: nickel foam collection The method of fluid early stage pretreatment, the method preparing nickel oxide/graphene combination electrode, test described combination electrode capacitive property Method
It is characterized in that, comprise the following steps:
(1) pretreatment of nickel foam collector (NF): nickel foam is cut into the square of certain size, is sequentially placed into acetone The ultrasonic certain time with in hydrochloric acid, thoroughly dry up with nitrogen after washing;
(2) configuring the PBS of certain pH, add a certain amount of graphene oxide, ultrasonic disperse uniformly obtains stablizing equal The graphene oxide suspension of one, with this solution as electrolyte, pretreated nickel foam collector is working electrode, builds three Electrode system, obtains reduced graphene by potentiostatic method at nickel foam collection liquid surface, builds graphene modified electrode;
(3) in the acetum of pH 4.0, certain density Ni (NO is configured3)2Solution, with it as electrolyte, Graphene is repaiied Decorations electrode is working electrode, builds three-electrode system, is obtained in graphene modified electrode surface electro-deposition by cyclic voltammetry Intermediate, is then replaced by the PBS solution of pH 7 by electrolyte, resets cyclic voltammetric sedimentary condition and obtains at electrode surface Nickel oxide nano sheet, takes out and i.e. can get nickel oxide/graphene combination electrode after drying;
(4) with KOH solution as electrolyte, with nickel oxide/graphene combination electrode as working electrode, three-electrode system is built, Cyclic voltammetry under research different scanning speed, the constant current charge-discharge under different electric current densities is tested and close at big electric current Constant current cycle charge discharge electrical testing under Du.
Have the most according to claim 1 the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic preparation method and Application, it is characterised in that: the nickel foam areal extent described in step 1 is 1 cm × 1 cm~10 cm × 10 cm;In step 1 Described concentration of hydrochloric acid is 1.0 mol/L~6.0 mol/L;Nickel foam porosity described in step 1 is more than 90%;In step 1 Described nickel foam pore diameter range is 1 mm ~ 10 mm.
Have the most according to claim 1 the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic preparation method and Application, it is characterised in that: the pH scope of the PBS described in step 2 is 3.0~8.0;The oxidation stated in step 2 The concentration range of Graphene is 0.5 mg/mL~5.0 mg/mL;The potentiostatic electrodeposition of the graphene oxide stated in step 2 Condition is: the excursion of sedimentation potential is-1.0 V~-1.5 V, and the excursion of sedimentation time is 50 s~1000 s;The three-electrode system stated in step 2 includes working electrode (nickel foam collector), reference electrode (saturated calomel electrode) With auxiliary electrode (platinum plate electrode).
Have the most according to claim 1 the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic preparation method and Application, it is characterised in that: the concentration of the nickel nitrate solution described in step 3 is 0.1 mmol/L~0.1 mol/L;In step 3 Described three-electrode system includes working electrode (graphene modified electrode), reference electrode (saturated calomel electrode) and auxiliary electrode (platinum plate electrode);The cyclic voltammetric sedimentary condition obtaining intermediate described in step 3 is potential window-1.0 V~0.5 V, Scanning speed 70 mV/s, the scanning number of turns is 30 circles;The sedimentary condition obtaining nickel oxide nano sheet stated in step 3 is electricity Position window-1.0 V~1.5 V, scanning speed 100 mV/s, the scanning number of turns is 30 circles.
Have the most according to claim 1 the nickel oxide/graphene combination electrode of electrochemical capacitance energy storage characteristic preparation method and Application, it is characterised in that: the concentration of the KOH solution described in step 4 is 1.0 mol/L;Three-electrode system described in step 4 For: with nickel oxide/graphene combination electrode as working electrode, hydrargyrum/mercuric oxide electrode is reference electrode, and platinum plate electrode is auxiliary electricity Pole;The potential range of the cyclic voltammetry curve described in step 4 is: 0~0.8 V;Different scanning speed described in step 4 is 5, 10, 20, 30, 50, 80, 100, 150 mV/s;The potential range of the charge-discharge test described in step 4 be 0~ 0.5 V;Different electric current densities described in step 4 are 1,2,3,5,10,20,40 mA/cm2
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CN107967997A (en) * 2017-11-28 2018-04-27 中国科学院深圳先进技术研究院 A kind of three-dimensional high heat-conductivity conducting composite material, its preparation method and application
CN108172407A (en) * 2017-12-26 2018-06-15 安徽大学 A kind of combination electrode, preparation method and application
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CN111540914A (en) * 2020-05-11 2020-08-14 辽宁大学 Preparation method of functional porous graphene integrated electrode material and application of functional porous graphene integrated electrode material in vanadium battery
CN113394030A (en) * 2021-06-26 2021-09-14 南昌师范学院 Nickel-based electrode material and preparation method and application thereof
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